化工社化工社 化学情報印刷レポート · 研究参考用
Benzoic acid, 3,5-dibromo- → 3,5-dibromo-N-cyclopropylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzoic acid, 3,5-dibromo- | HCID 12063 | — |
| 反応物 | Cyclopropylamine | HCID 69828 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3,5-dibromo-N-cyclopropylbenzamide | HCID 67062088 | — |
反応手順
To a stirred solution of 3,5-dibromobenzoic acid (1 eq.) in DMF (0.15 M) was added HATU (1.3 eq.), cyclopropylamine (1.1 eq.) and Hunig's base (3 eq.). The resulting yellow mixture was stirred at RT for 18 h. The reaction was then quenched with saturated aqueous ammonium chloride and extracted with ethyl acetate. The combined organic extracts were washed further with water and brine, dried over Na2SO4, filtered and the filtrate concentrated in vacuo. Trituration of the crude product thus obtained in a mixture of ether and hexanes afforded the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08889714B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-3e4244c5b4c2486dbba4e4862f388986 |
| 出典メモ | uspto-grants-2014_11 |